The research proposed in this application is aimed towards the application of recently developed techniques in vibrational spectroscopy and vibrational optical activity to the study of solution conformation of peptides. The rational behind these efforts can be summarized as follows: first, existing experimental techniques to study peptide solution conformation for very small, flexible peptides are somewhat limited and thus, the availability of conformational data from different techniques would be a welcome improvement. Second, the techniques to be utilized in the proposed research have been developed and described in detail; however, their application to real problems in structural chemistry has been delayed due to the difficulties in obtaining biochemically significant, yet sufficiently simple, sample systems, and due to the problems in the interpretation of experimental results. The research described in the following proposal addresses these points in detail, and both the synthesis of a series of stereo-selectively, deuterated peptides via solid state methods as well as detailed vibrational analysis of peptides have been intiated. Instrumentation for the observation of Raman Differences Spectra has been completed, and Raman Optical Activity capabilities will be available in ca. six months. This application requests funds to provide the necessary man power for the continuation of these efforts and to improve present instrumental capabilities.